US5614248A
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Method for plasma-assisted reactive electron beam vaporization
Assignee: Fraunhofer-Gesellschaft zur Förderung der Angewandten Forschung eV
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Filing: 1993-08-18
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Granted: 1997-03-25
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Expires: 2013-08-18
Abstract
Abstract Certain non-optical characteristics and, in particular, mechanical characteristics are not measurable in situ in the industrial production of layers using plasma-assisted reactive electron beam vaporization, particularly if high demands are made on the hardness, wear resistance and barrier action, so as to be able to reproducibly apply the layers. The values of the optical layer characteristics are to be used as a control signal. In this method, immediately after the substrate has passed through the vaporizing zone, the reflection and/or transmission and absorption capacity are measured in the wavelength range Δ k =150 to 800 nm and from this are determined the refractive index and optical absorption coefficient. These determined values are compared with an experimentally determined desired value. A control signal obtained therefrom, in the case of a constant reactive gas partial pressure, controls the plasma and maintains constant the optical characteristics of the layer. The method is used in the vapor-deposition of wear-resistance, hard layers or barrier layers, e.g. of metal oxide on glass, plastic and other materials, e.g. in the building industry for facade glass and in the packaging industry.
Inventors
- 👤 Siegfried Schiller
- 👤 Manfred Neumann
- 👤 Volker Kirchhoff
- 👤 Gerhard Zeissig
- 👤 Nicolas Schiller
- 👤 Klaus Goedicke
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 10:39
CPC Classifications
C; C23; C23C; C23C14/00; C23C14/22; C23C14/54; C23C14/0021
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
252 words
A method for coating a substrate with a layer having defined mechanical characteristics by plasma-assisted reactive electron beam vaporization producing a controllable plasma in a process zone between a vaporizing material and the substrate so as to deposit a coating layer on said substrate, and providing in situ measurement of optical characteristics of the coating layer deposited on the substrate, the method comprising the steps of: experimentally determining a correlation between optical characteristics and mechanical characteristics of the coating layer; measuring in a wavelength range Δ k =150 nm to 800 nm at least one of a reflection, transmission and absorption capacity of the coating layer on the substrate immediately after the substrate passes through a vaporizing zone; separately determining from said measuring step a refractive index n and an optical absorption coefficient k; deriving initial mechanical characteristics of the coating layer corresponding to said index n and said coefficient k; comparing said derived initial mechanical characteristics with the defined mechanical characteristics to obtain a control signal; and using the control signal to control operating parameters of the plasma in a case of a constant reactive gas partial pressure in such a manner that said measured optical characteristics of the coating layer are maintained constant to achieve the defined mechanical characteristics, and in a case of constant plasma parameters, using the control signal to control the reactive gas partial pressure in such a manner that the measured optical characteristics of the coating layer are kept constant to achieve the defined mechanical characteristics.
Claim 2
Independent Claim
252 words
A method for coating a substrate with a layer having defined mechanical characteristics by plasma-assisted reactive electron beam vaporization producing a controllable plasma in a process zone between a vaporizing material and the substrate so as to deposit a coating layer on said substrate, and providing in situ measurement of optical characteristics of the coating layer deposited on the substrate, the method comprising the steps of: experimentally determining a correlation between optical characteristics and mechanical characteristics of the coating layer; measuring in a wavelength range Δ k =150 nm to 800 nm at least one of a reflection, transmission and absorption capacity of the coating layer on the substrate immediately after the substrate passes through a vaporizing zone; separately determining from said measuring step a refractive index n and an optical absorption coefficient k; deriving initial mechanical characteristics of the coating layer corresponding to said index n and said coefficient k; comparing said derived initial mechanical characteristics with the defined mechanical characteristics to obtain a control signal; and using the control signal to control operating parameters of the plasma in a case of a constant reactive gas partial pressure in such a manner that said measured optical characteristics of the coating layer are maintained constant to achieve the defined mechanical characteristics, and in a case of constant plasma parameters, using the control signal to control the reactive gas partial pressure in such a manner that the measured optical characteristics of the coating layer are kept constant to achieve the defined mechanical characteristics.
Claim 3
Dependent Claim
48 words
Method according to claim 1, wherein for ensuring a fundamental stability of a plasma generating source, an intensity of a plasma emission in the process zone is measured and an operation of the plasma generating source is regulated by regulating one of an electric power and gas flow.
Claim 4
Dependent Claim
19 words
Method according to claim 1, wherein the reactive gas partial pressure is regulated by regulating a reactive gas flow.
Claim 5
Dependent Claim
22 words
Method according to claim 1, wherein the reactive gas partial pressure is regulated by regulating a suction capacity of a vacuum pump.
Claim 6
Dependent Claim
29 words
A method according to claim 1, wherein the mechanical characteristics are related to at least one of a hardness, a wear-resistance, and a barrier action of said coating layer.
Claim 7
Dependent Claim
24 words
A method according to claim 1, further comprising the step of using one of a glass material and a plastic material as said substrate.
Claim 8
Dependent Claim
25 words
A method according to claim 1, further comprising the step of operating said plasma-assisted reactive electron beam vaporization at a coating rate of 0.5 μm/s.
Claim 9
Dependent Claim
26 words
A method according to claim 1, further comprising the step of operating said plasma-assisted reactive electron beam vaporization at a coating rate of about 800 nm/s.
Claim 10
Independent Claim
218 words
A method for coating a substrate with a wear-resistant layer and/or a layer with barrier characteristics by plasma-assisted reactive electron beam vaporization producing a controllable plasma in a process zone between a vaporizing material and the substrate to be coated, and providing in situ measurement of optical characteristics of the coating layer deposited on the substrate, the method comprising the steps of: measuring in a wavelength range Δ k =150 nm to 800 nm at least one of a reflection, transmission and absorption capacity of the coating layer on the substrate immediately after the substrate passes through a vaporizing zone; separately determining from said measuring step a refractive index n and an optical absorption coefficient k; comparing said values n and k with an experimentally determined value corresponding to a predetermined wear-resistant layer and/or a predetermined layer with barrier characteristics to obtain a control signal; and using the control signal to control operating parameters of the plasma in a case of a constant reactive gas partial pressure in such a manner that said measured optical characteristics of the coating layer are maintained constant, and in a case of constant plasma parameters, using the control signal to control the reactive gas partial pressure in such a manner that the measured optical characteristics of the coating layer are kept constant.
Claim 11
Independent Claim
218 words
A method for coating a substrate with a wear-resistant layer and/or a layer with barrier characteristics by plasma-assisted reactive electron beam vaporization producing a controllable plasma in a process zone between a vaporizing material and the substrate to be coated, and providing in situ measurement of optical characteristics of the coating layer deposited on the substrate, the method comprising the steps of: measuring in a wavelength range Δ k =150 nm to 800 nm at least one of a reflection, transmission and absorption capacity of the coating layer on the substrate immediately after the substrate passes through a vaporizing zone; separately determining from said measuring step a refractive index n and an optical absorption coefficient k; comparing said values n and k with an experimentally determined value corresponding to a predetermined wear-resistant layer and/or a predetermined layer with barrier characteristics to obtain a control signal; and using the control signal to control operating parameters of the plasma in a case of a constant reactive gas partial pressure in such a manner that said measured optical characteristics of the coating layer are maintained constant, and in a case of constant plasma parameters, using the control signal to control the reactive gas partial pressure in such a manner that the measured optical characteristics of the coating layer are kept constant.
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| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 2000-03-24 | 2000-09-23 | 2001-03-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2004-03-24 | 2004-09-23 | 2005-03-25 | $3760.00 | Window Closed / Lapsed |
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